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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Design and Development of Novel Equiatomic Refractory Multi Principal elemental Alloys Based on MoNbTi System for Use in Irradiation Environments

Multi Principal Elemental Alloys (MPEA) have emerged as promising materials for next-generation nuclear reactors due to their exceptional irradiation resistance. Eight equiatomic MPEA based on the MoNbTi system, comprising of elements with low thermal neutron absorption cross-sections were explored using a combined approach employing empirical parameter estimations, and CALPHAD simulations by which the phases and elemental segregation observed in all the alloys in the as-cast state were predicted. Solution heat treatment at 1500°C transformed five alloys into single-phase matrix materials, enhancing homogeneity and reducing hardness. The densities of the alloys ranged between 6.47 to 7.68 g/cm3, hardness between 472 and 656 VHN, Young’s modulus between 142 GPa to 169 GPa, shear modulus between 54 GPa and 62 GPa, bulk modulus between 117 GPa to 194 GPa and Poisson’s ratio between 0.3 to 0.35. The in-situ high temperature Xray diffraction results, differential scanning calorimetry and dilatometry results up to 1000°C suggested the high temperature phase stability of the MPEA. Subsequent ageing heat treatment at 800 and 1000 oC for 96 hours revealed significant secondary phase precipitation in MoNbTiZr, MoNbTiZrV, and MoNbTiCrA. Oxidation studies at 800 oC for 24 hours in air revealed superior oxidation resistance and cubic rate law dependence in Cr containing MPEA especially in MoNbTiCrAl, while severe mass gain resulting in total disintegration and exfoliation in MoNbTiZr and MoNbTiZrV. This comprehensive study underscores the potential of novel MPEA as promising materials for advanced nuclear reactor applications, shedding light on their microstructural control, mechanical properties, thermal stability, and oxidation resistance.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

In-situ synchrotron X-ray diffraction of hydroxyapatite-zirconia composite during conventional and flash sintering

Here, we conducted in-situ X-ray diffraction to study the crystalline phase evolution in hydroxyapatite-zirconia composites during both conventional and flash sintering processes. Additionally, we examined the thermal history and microstructure of the composite under these sintering conditions. Despite both sintering methods reaching similar average temperatures, they yielded distinct results in terms of crystalline phase composition and microstructure. In the flash sintered samples, we observed a complete transformation of hydroxyapatite into α- tricalcium phosphate and a complete tetragonal to cubic phase transition in zirconia. Conversely, the conventionally sintered samples remained practically stable. Notably, the flash sintered samples exhibited needle-like microstructures, which were absent in their conventionally sintered counterparts. This divergence suggests that the application of an electric field plays a role in generating athermal effects during the sintering of hydroxyapatite-zirconia composites.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Ohm’s Law, the Reconnection Rate, and Energy Conversion in Collisionless Magnetic Reconnection

Magnetic reconnection is a ubiquitous plasma process that transforms magnetic energy into particle energy during eruptive events throughout the universe. Reconnection not only converts energy during solar flares and geomagnetic substorms that drive space weather near Earth, but it may also play critical roles in the high energy emissions from the magnetospheres of neutron stars and black holes. In this review article, we focus on collisionless plasmas that are most relevant to reconnection in many space and astrophysical plasmas. Guided by first-principles kinetic simulations and spaceborne in-situ observations, we highlight the most recent progress in understanding this fundamental plasma process. We start by discussing the non-ideal electric field in the generalized Ohm’s law that breaks the frozen-in flux condition in ideal magnetohydrodynamics and allows magnetic reconnection to occur. We point out that this same reconnection electric field also plays an important role in sustaining the current and pressure in the current sheet and then discuss the determination of its magnitude (i.e., the reconnection rate), based on force balance and energy conservation. This approach to determining the reconnection rate is applied to kinetic current sheets with a wide variety of magnetic geometries, parameters, and background conditions. We also briefly review the key diagnostics and modeling of energy conversion around the reconnection diffusion region, seeking insights from recently developed theories. Finally, future prospects and open questions are discussed.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2025

Status Report on Design of In-situ Thermomechanical Testing at LANSCE

Nuclear fuel encounters severe thermomechanical environments in which its mechanical response is determined by its microstructure, temperature and stress level histories. Simulating the response of such microstructures is crucial for predicting both performance and transient fuel mechanical responses and experimental verification of such predictions is therefore of great interest. While most of the deformation in a nuclear fuel rod occurs in the cladding, deformation of the fuel itself is still of interest with deformation mechanisms at operating temperature and above including creep, swelling, cracking as well as pellet-clad interaction. Characterization of these properties and understanding of the underlying deformation phenomena at operating or excursion temperatures is therefore of great importance for development and ultimately licensing of improved and novel nuclear fuel forms. Diffraction techniques offer unique insight on the atomistic (e.g. crystal structure) and microstructure (e.g. phase transformations, texture, defects) length scales and have a long history of providing unique data to inform relevant deformation models that enable the required predictive capabilities. For example, dislocations lead to diffraction peak broadening that can be characterized to estimate the dislocation density and study the role of dislocations on the deformation while measuring lattice strains allows to studie load sharing in two phase materials. In this report the requirements for a sample environment for high temperature deformation of nuclear fuels are defined. The HIPPO neutron time-of-flight diffractometer at LANSCE will host this sample environment and is also described. This instrument covers diffraction angles from 140° to 40° and is also equipped with an event-mode neutron imaging detector system, enabling energy-resolved neutron imaging in parallel with the diffraction that could measure sample temperature from Doppler broadening of neutron absorption resonances or measure pore densities from changes in the attenuation. Designs of devices to characterize thermomechanical properties of nuclear fuel without diffraction are also considered to guide the design. While this report is focused on applications for nuclear fuels, the device can also characterize cladding, moderator or structural materials and therefore contribute to other fields of research and development for advanced reactors. The temperatures planned to be reached are above 2000℃, thus enabling characterization of LWR reactor fuels under accident scenarios but also reaching temperatures of fuels developed for nuclear thermal propulsion and providing opportunities to characterize those. In conjunction with the energy-resolved neutron imaging detector, this setup would allow to measure neutron cross-sections at high temperatures, filling a gap towards development of reactors operating at high temperatures.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Application of Ibuprofen Sodium Dihydrate for Thermochemical Energy Storage

Thermochemical energy storage (TCES) offers a transformative approach to address grid instability by harnessing reversible chemical reactions for efficient heat storage and release. Here, we introduce pharmaceutical organic salt hydrates as a class of materials with exceptional performance for low-grade waste heat recovery. We demonstrate ibuprofen sodium dihydrate (ISD) as an example organic hydrate exhibiting a dehydration temperature range of 60-110 °C and a remarkable dehydration enthalpy of up to 59.5 kJ/mol of water, ideally suited for capturing industrial and residential waste heat. Using rigorous multimodal characterization, including thermogravimetric analysis, differential scanning calorimetry, in-situ FTIR, in-situ PXRD, and NMR, we demonstrate ISD's superior thermal, chemical, and structural stability over 150 hydration-dehydration cycles, achieving an unprecedented cycling efficiency of ~99.9%. Compared to conventional inorganic salt hydrates like strontium chloride hexahydrate and calcium oxalate monohydrate, ISD showcases enhanced durability without deliquescence or pulverization, even under high-humidity conditions. In-situ analyses confirm the transition from ISD to ibuprofen sodium anhydrous (ISA) proceeds with structural reorganization, thereby combining the dehydration mechanism with phase transitions, resulting in higher energy storage capacity. Microstructural analyses reveal that repeated water intercalation and structural transitions aid in creating significant porosity that enhances water transport kinetics, further improving the hydration/dehydration performance. By combining the phase change and chemical dehydration mechanisms, ISD paves the way for designing a new class of organic salt hydrates, offering tunable properties to meet diverse thermal energy storage demands and supporting sustainable grid resilience.

Thangaraj, Kavin C.↗
DOE OSTI2025

Ultralow-temperature cryogenic transmission electron microscopy using a new helium flow cryostat stage

Advances in cryogenic electron microscopy have opened new avenues for probing quantum phenomena in correlated materials. This study reports the installation and performance of a new side-entry condenZero cryogenic cooling system for JEOL (Scanning) Transmission Electron Microscopes (S/TEM), utilizing compressed liquid helium (LHe) and designed for imaging and spectroscopy at ultra-low temperatures. The system includes an external dewar mounted on a vibration-damping stage and a pressurized, low-noise helium transfer line with a remotely controllable needle valve, ensuring stable and efficient LHe flow with minimal thermal and mechanical noise. Performance evaluation demonstrates a stable base temperature of 4.37 K measured using a Cernox bare chip sensor on the holder with temperature fluctuations within ±0.004 K. Complementary in-situ electron energy-loss spectroscopy (EELS) via aluminum bulk plasmon analysis was used to measure the local specimen temperature and validate cryogenic operation during experiments. The integration of cryogenic cooling with other microscopy techniques, including electron diffraction and Lorentz TEM, was demonstrated by resolving charge density wave (CDW) transitions in NbSe2 using electron diffraction, and imaging nanometric magnetic skyrmions in MnSi via Lorentz TEM. In conclusion, this platform provides reliable cryogenic operation below 7 K, establishing a low-drift route for direct visualization of electronic and magnetic phase transformations in quantum materials.

Charge density wave↗
DOE OSTI2026

Model-based, in-situ, non-destructive qualification and certification of parts made by autonomous additive manufacturing

To address the significant productivity challenges associated with the qualification and certification (Q&C) tasks of additively manufactured (AM) parts, which have traditionally relied on rigorous post‐build inspection and testing, we propose an integrated framework that combines model‐based qualification and certification (MBQ&C) with autonomous additive manufacturing (AAM). MBQ&C employs high‐fidelity predictive models, developed within the Integrated Computational Materials Engineering (ICME) paradigm, to simulate process–structure–property–performance relationships for assessing a part’s fitness for use. Since predictive models are commonly machine learning (ML)-based or reduced-order surrogates of validated physics models, they run efficiently, enabling timely inference. In parallel, the self-driving AAM utilises ML-based adaptive, closed‐loop control strategies to avoid, mitigate, or repair defects and anomalies during fabrication, thereby increasing the likelihood of producing acceptable parts. A key feature of the combined AAM-MBQ&C framework is that predictive models explicitly incorporate defects or anomalies that persist after the build, using instance-specific data captured via in-situ sensing. This customisation enables a build‐specific assessment of fitness for use, rather than relying on nominal or generic parameters. Such individualised evaluation provides a robust basis for Q&C-related acceptance decisions relating to each build. Additionally, the rapid solution capabilities of ML or reduced-order models enable the determination of a part’s suitability for service shortly after build completion. As the framework matures, it has the potential to substantially reduce reliance on conventional point‐design approaches—such as time‐consuming post‐build computed tomography scanning and costly destructive testing. Thus, the AAM-MBQ&C framework represents a transformative, scalable strategy for quality assurance of AM components, as parts produced within a stable, validated, and certified envelope can be certified with reduced testing. Key benefits include: (1) significant gains in Q&C productivity through efficient, model-centric assessment; (2) performance-based classification of defects into critical and non-critical categories; (3) the ability to predict potential deviations in the performance of parts affected by real-time, adaptive process control interventions relative to those produced under a certified process, and (4) the enabling of virtual Q&C for service environments that are difficult, hazardous, or impractical to access or reproduce experimentally. Collectively, these capabilities strengthen the business case for AM, particularly for high‐consequence and mission‐critical applications. Finally, although this work focuses on powder-based AM, the proposed techniques could be extended to AM processes employing alternative feedstock forms.

Gunasegaram, Dayalan↗
DOE OSTI2024

Mechanisms of ion irradiation induced ordering in amorphous TiO 2 nanotubes: Effects of ion mass and energy

Here, amorphous TiO 2 nanotubes were irradiated in-situ in a transmission electron microscope (TEM) with Kr + ions at energies of 46 keV, 150 keV, and 1 MeV and with 46 keV Xe + ions, to investigate the structural and morphological evolution of the nanotubes under irradiation. At all irradiation conditions, amorphous TiO 2 nanotubes exhibited significant morphological instability, and tended to undergo volumetric swelling with increasing ion counts, often until collapse of the original nanotube structure. Molecular dynamics (MD) simulations confirmed that irradiation-induced defects can explain the observed swelling. Structurally, nanotubes remain amorphous following all Kr + irradiation conditions, but irradiation with 46 keV Xe + leads to the formation of anatase nanocrystallites. Importantly, through systematically varying ion energy and ion species, we try to elucidate the influence of nuclear and electronic stopping power on ion irradiation induced changes. By contextualizing these results within the existing literature, we propose that the observed changes in TiO 2 nanotube morphology and structure could be due to a competition between two mechanisms: (1) disorder-induced swelling and (2) irradiation-induced amorphous-to-crystalline transformation.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Transient Studies of CO 2 Adsorption over CeO 2 Nanostructures with In Situ DRIFTS and Modulation Excitation

Experiments of in-situ DRIFTS combined with modulation excitation (ME) spectroscopy showed a rich surface chemistry associated with the adsorption of CO 2 on nanocubes and nanospheres of ceria. The nanocubes exposed faces with a (100) orientation, with the edges and corners displaying (110) and (111) orientations, respectively. Here, the nanospheres mainly contained ceria (111) and (110) planes. DFT calculations showed that CO 2 is a multidentate adsorbate on ceria that can undergo changes in its bonding configuration depending on the chemical environment. At 250 °C, a temperature typically used for the conversion of CO 2 into oxygenates, alkanes and olefins, CO 2 reacted with O centers or OH groups present on the nanocubes and nanospheres to yield bi- and tri-dentate carbonates, hydroxycarbonates, and formates. Both nanostructures were highly reactive and a dynamic equilibrium was established: carbonate species were rapidly generated upon the injection of CO 2 and they decomposed upon the removal of CO 2 from the gas phase. In the case of the ceria nanocubes, the adsorption/desorption processes were essentially reversible, opening the door to catalytic transformations. A larger concentration of defects in the ceria nanospheres led to strongly bound carbonates and formates that may be spectators, site blockers, or surface modifiers in catalytic processes. In the ME studies, additional intermediates were detected, and it was clear that the response of surface species to the presence/absence of CO 2 was highly dependent on the morphology of the ceria nanostructures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Atomistic Mechanisms of the Crystallographic Orientation‐Dependent Cu 1.8 S Conductive Channel Formation in Cu 2 S‐Based Memristors

Achieving multiple types of resistive switching in a single material with controlled ionic motion is a key challenge in neuromorphic computing, traditionally addressed by combining materials with distinct switching behaviors. Here, Cu 2-x S is identified as a promising candidate to overcome this limitation due to its hierarchical phase transitions. Using in situ biasing experiments, reversible and non-reversible phase transitions (and resistive switching) are demonstrated in γ-Cu 2 S by controlling the compliance current. The formation of parallel high-digenite Cu 1.8 S channels, orientated along the γ-Cu 2 S [201] crystallographic direction, drives the nonvolatile resistive switching. These channels emerge via an intermediate δ-Cu 2 S phase and are stabilized at room temperature by residual strains, alongside β-Cu 2 S phase. In conclusion, the work clarifies the complex, electrically triggered phase transformations in γ-Cu 2 S, and highlights the potential of Cu 2-x S as a versatile material for neuromorphic computing.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2024

Crystal structure solution and high-temperature thermal expansion in NaZr 2 (PO 4 ) 3 -type materials

The NaZr 2 P 3 O 12 family of materials have shown low and tailorable thermal expansion properties. In this study, SrZr 4 P 6 O 24 (SrO·4ZrO 2 ·3P 2 O 5 ), CaZr 4 P 6 O 24 (CaO·4ZrO 2 ·3P 2 O 5 ), MgZr 4 P 6 O 24 (MgO·4ZrO 2 ·3P 2 O 5 ), NaTi 2 P 3 O 12 [½(Na 2 O·4TiO 2 ·3P 2 O 5 )], NaZr 2 P 3 O 12 [½(Na 2 O·4ZrO 2 ·3P 2 O 5 )], and related solid solutions were synthesized using the organic–inorganic steric entrapment method. The samples were characterized by in-situ high-temperature X-ray diffraction from 25 to 1500°C at the Advanced Photon Source and National Synchrotron Light Source II. The average linear thermal expansion of SrZr 4 P 6 O 24 and CaZr 4 P 6 O 24 was between −1 × 10 −6 per °C and 6 × 10 −6 per °C from 25 to 1500°C. The crystal structures of the high-temperature polymorphs of CaZr 4 P 6 O 24 and SrZr 4 P 6 O 24 with R 3 c symmetry were solved by Fourier difference mapping and Rietveld refinement. This polymorph is present above ∼1250°C. This work measured thermal expansion coefficients to 1500°C for all samples and investigated the differences in thermal expansion mechanisms between polymorphs and between compositions.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Develop an efficient and cost-effective novel anaerobic digestion system producing high purity of methane from diverse waste biomass

This project focuses on developing an advanced, intensified anaerobic digestion system aimed at transforming the treatment and conversion of organic wastes into valuable products, specifically renewable natural gas. The motivation for this research stems from the limitations of conventional anaerobic digestion technologies, which often face challenges such as long retention times, high operational costs, and incomplete organic material degradation. The new technology called Intensified Versatile Anaerobic Digestion (IVAD), is developed to address these challenges by incorporating innovative reactors and processes that enhance the overall efficiency and output of anaerobic digestion. The significance of this project lies in its potential to revolutionize waste management practices and waste biomass utilization. The IVAD system integrates a hyperthermophilic anaerobic acidification reactor, a hydrothermal treatment (HTT) unit, and both thermophilic and mesophilic methanogenic reactors. This combination enables a higher rate of organic breakdown and energy recovery, resulting in faster processing times, reduced reactor sizes, and lower operational costs compared to traditional systems. Key data include an increase in methane productivity to 1.18 m 3 /m 3 /day, a significant improvement compared to the baseline technology’s 0.64 m 3 /m 3 /day. Additionally, the IVAD system achieves a 45% reduction in levelized cost of energy (LCOE), down to $\$$10.04/MMBTU, and an energy return on investment (EROI) of 3.19, representing an 87% increase over baseline levels. Technical and economic analyses highlight that the IVAD system significantly reduces hydraulic retention time (HRT) and solid retention time (SRT). The HRT for the HTT reactor can be reduced from 1 hour to 0.5 hours, while decoupling SRT from HRT in the anaerobic acidification reactor (AAR) allows for further reductions. These design optimizations lead to smaller reactor volumes, cutting down equipment and construction costs. Despite these advancements, energy consumption remains comparable to conventional methods due to a novel heat recovery strategy, enhancing overall process productivity. The system also achieves in-situ CO 2 removal and ammonia stripping features, resulting in biogas with a methane purity level of 75%, and produces high-quality nitrogen fertilizer as an additional by-product. Public benefits of the IVAD system are substantial, contributing to sustainable waste management and renewable energy production. By providing a scalable solution that can be adopted by dairy farms and similar agricultural operations, the IVAD system helps reduce waste, produce renewable natural gas (RNG) suitable for transportation fuel, and generate fertilizer, supporting a circular economy. This project plays a role in achieving broader environmental objectives by mitigating greenhouse gas emissions and promoting energy independence. Additionally, it offers a pathway for farmers to lower operational costs while adopting practices that are both environmentally sustainable and economically advantageous.

03 NATURAL GAS↗
DOE OSTI2025

Enhancing carbon nanotube production from carbon dioxide and ethane using bimetallic catalysts

Converting CO 2 into carbon nanotubes (CNTs) offers a promising way for CO 2 utilization and sequestration, potentially mitigating environmental impacts from anthropogenic emissions. This study reports that bimetallic CoFe catalysts can increase CNT production from the reaction of CO 2 and C 2 H 6 by an order of magnitude compared to their monometallic counterparts. The active sites and CNT morphologies are composition-dependent: Co-rich catalysts (Co/Fe ratio ≥ 5) form stable face-centered cubic (fcc) CoFe alloys, producing cylindrical CNTs; Fe-containing catalysts (Co/Fe ≤ 2) favor body-centered cubic (bcc) CoFe alloy upon reduction, which transforms into carbides, resulting in bamboo-like CNTs. Experimental evidence and DFT calculations reveal that adjacent Fe and Co atoms modulate CO and C x H y adsorption, regulating CNT production pathways through the CO Boudouard reaction and C 2 H 6 decomposition. In conclusion, these results highlight the dual benefits of bimetallic catalysts in enhancing CNT yield and controlling CNT morphology through adjustment of catalyst compositions.

58 GEOSCIENCES↗
DOE OSTI2025

Defect-Driven Redox Interplay on Anatase TiO 2 : Surface-Structure Dependent Activation for CO 2 Hydrogenation Catalysis

Titanium dioxide (TiO 2 ) is one of the most extensively studied oxides as an active catalyst or catalyst support, particularly in energy and environmental applications, but the atomistic mechanisms governing its dynamic response to reactive environments and their correlation to reactivity remain largely elusive. Using in situ environmental transmission electron microscopy (ETEM), synchrotron X-ray diffraction (XRD), ambient-pressure X-ray photoelectron spectroscopy (AP-XPS), temperature-programmed reduction (TPR), reactivity measurements, and theoretical modeling, we reveal the dynamic interplay between oxygen loss and replenishment of anatase TiO 2 under varying reactive conditions. Under H 2 exposure, anatase TiO 2 undergoes surface reduction via lattice oxygen loss, forming Ti 3 O 5 . In contrast, CO 2 exposure induces oxygen replenishment, reversing stoichiometry. In mixed H2/CO 2 environments, the reverse water–gas shift (RWGS) reaction proceeds selectively on stepped and high-indexed TiO 2 surfaces, whereas the thermodynamically stable TiO 2 (101) surface remains inactive and intact. Critically, H 2 pretreatment generates oxygen vacancies on TiO 2 (101), transforming it into an active Ti 3 O 5 or defect-rich surface that catalyzes RWGS. By correlating surface structure, defect dynamics, and gas-phase interactions, this work deciphers the competition between H 2 -driven reduction and CO 2 -driven oxidation pathways at the atomic scale. Furthermore, these insights establish defect engineering as a strategic lever to activate inert TiO 2 facets, advancing the design of adaptive catalysts for sustainable fuel synthesis technologies.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Activity and selectivity for CO 2 methanation of clusters and nanoplates of ruthenium dispersed on ceria: In-situ studies with XAFS and DRIFTS

The performance of Ru/CeO 2 catalysts under CO 2 hydrogenation conditions was studied using in situ X-ray absorption fine structure (XAFS) and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) to understand the structural evolution and chemical nature of each component under reaction conditions. The catalysts were prepared using a reverse microemulsion method that maximized the dispersion of RuOx particles on ceria. A RuO x → Ru transformation was observed upon exposure of the RuO x /CeO 2 systems to H 2 at 250 °C. For a sample with 5% molar Ru, two-dimensional clusters (2-4 atoms) of Ru formed on top of the ceria support. An increase in the loading of ruthenium to 20% molar led to the formation of nanoplates of the metal 2-3 atomic layers thick. Both Ru structures were highly dispersed on ceria. They were oxidized after exposure to CO 2 at 250 °C. However, under CO 2 /H 2 mixture, they remained in a metallic state as two-dimensional clusters and nanoplates. In situ DRIFTS studies, the 5% and 20% Ru/CeO 2 catalysts showed distinct reaction intermediates when exposed to CO 2 or CO 2 /H 2 (1/4) reaction mixtures. Normalized to the Ru molar percentage, the 5% Ru/CeO 2 system was the most active catalyst exhibiting a selectivity of ~ 60% CH 4 and 40% CO at 250 °C. On the other hand, under the same reaction conditions, the 20% Ru/CeO 2 system was less active but had a CH 4 selectivity close to 80%. In conclusion, these results highlight the importance of the structure of the metallic Ru particles as a factor that determines the catalytic performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

In situ high-temperature Raman spectroscopy for online EAF slag analysis

Real-time monitoring of slag chemistry is critical for optimizing Electric Arc Furnace (EAF) steelmaking operations, where dynamic variations in slag composition directly influence slag foaming, refractory degradation, and thermal efficiency. Conventional techniques such as X-ray fluorescence (XRF), Fourier-transform infrared (FTIR), and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDS) are commonly used to analyze slag composition, but their offline nature and equipment constraints limit their applicability for online monitoring in harsh industrial environments. To address this challenge, we present an in situ, high-temperature analytical approach that integrates Raman spectroscopy with a custom designed fiber-optic probe for real-time slag characterization at 1550 °C. The system enables non destructive spectral acquisition from molten slags, providing molecular-level insights into silicate polymerization and iron oxidation states. Eight synthetic slag samples were evaluated, and key Raman features—such as Q n silicate units and FeO₄/FeO₆ coordination environments—were identified and quantitatively correlated with slag basicity and Fe₂O₃ content. The results demonstrate agreement between Raman spectral ratios and bulk slag chemistry, validating the method’s capability to track compositional and structural changes under molten temperature. This work establishes the feasibility of deploying fiber-optic Raman probe for online EAF slag monitoring and highlights their potential to support closed-loop control strategies, thereby enhancing process stability, refractory protection, and steel quality in industrial steelmaking applications.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

Synergistic effects of Pd single atoms and nanoclusters boosting SnO 2 gas sensing performance

Tin(IV) oxide-supported Pd is a promising heterogenous catalyst for CO oxidation relevant for environmental cleanup reactions. In this study, an atomically dispersed Pd catalyst on SnO 2 (ADC Pd/SnO 2 ) hybrid material is successfully synthesized via a straightforward wet chemistry method and is found to exhibit superior performance toward CO sensing. Ex situ EXAFS analysis confirms the formation of single Pd atoms and small Pd nanoclusters stabilized on the SnO 2 (110) surface. Further, the material exhibits high efficiency in generating adsorbed O 2 - as well as high activity in catalyzing CO oxidation at low temperatures, resulting in exceptional sensitivity and selectivity toward CO in comparison to pure SnO 2 and Pd nanoparticles loaded on SnO 2 respectively. In situ FTIR measurements unravel CO adsorption kinetics on ADC Pd/SnO 2 under reaction conditions, and a possible sensing mechanism is put forth in which CO is transformed into CO 2 by reaction with active oxygen species; and concurrently, carbon-related species (bicarbonates and carbonates) are formed and decomposed into CO 2 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Data for: Time to anoxia: Observations and predictions of oxygen drawdown following coastal flood events

This dataset contains data and code associated with the paper Patel et al. "Time to anoxia: Observations and predictions of oxygen drawdown following coastal flood events".The coastal terrestrial-aquatic interface (TAI) is a highly dynamic system characterized by strong physical, chemical, and biological gradients. In particular, shifting soil redox conditions and consumption of terminal electron acceptors, due in part to dynamic hydrologic conditions, is a strong driver of carbon availability and transformations across TAIs. However, while redox dynamics are well described, our ability to quantitatively forecast rates of oxic to anoxic shifts in soils with different characteristics and inundation regimes is limited. We integrated field measurements, laboratory incubations, and model simulations to improve mechanistic understanding of oxygen consumption dynamics in coastal soils. Continuous in situ monitoring unexpectedly revealed that flooding caused temporary spikes in subsurface dissolved oxygen followed by rapid consumption in the wetlands. To further investigate these mechanisms in a controlled setting, we performed laboratory incubations using surface and subsurface soils from a TAI gradient (defined here as upland forest to transitional forest to wetland) in Western Lake Erie to measure oxygen consumption rates in TAI soils during flood events. In our experiments, wetland soils reached anoxia the fastest, in ∼ 9 h on average, whereas upland soils turned anoxic in ∼ 18 h. Subsurface upland soils did not turn anoxic even after two weeks of saturation in the lab, and their oxygen consumption patterns suggested carbon and/or nutrient limitation. These results are consistent with in-situ groundwater redox and oxygen measurements in the field, where wetland soils exhibited the highest rates of oxygen consumption along the TAI. Model simulations of oxygen consumption suggested that oxygen consumption had stronger abiotic controls in wetland soils but stronger biotic controls in upland soils, providing a useful framework for future incubation experiments. Microbial activity is a strong driver of oxygen consumption in TAI soils, although it is constrained by the availability of dissolved carbon in subsurface soils.This dataset contains a compressed (.zip) archive of the data and R scripts used for this manuscript. The dataset includes files in .csv format, which can be accessed and processed using MS Excel or R. This archive can also be accessed on GitHub at https://github.com/COMPASS-DOE/cmps-time_to_anoxia (DOI: 10.5281/zenodo.10815374).

54 ENVIRONMENTAL SCIENCES↗